US7902288B2 - Sealant materials containing diblock copolymers and methods of making thereof - Google Patents

Sealant materials containing diblock copolymers and methods of making thereof Download PDF

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Publication number
US7902288B2
US7902288B2 US11/141,137 US14113705A US7902288B2 US 7902288 B2 US7902288 B2 US 7902288B2 US 14113705 A US14113705 A US 14113705A US 7902288 B2 US7902288 B2 US 7902288B2
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diblock copolymer
styrene
mineral oil
rubber
grease
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US20060270785A1 (en
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William V. Dower
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3M Innovative Properties Co
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3M Innovative Properties Co
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Assigned to 3M INNOVATIVE PROPERTIES COMPANY reassignment 3M INNOVATIVE PROPERTIES COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: DOWER, WILLIAM V.
Priority to TW095119283A priority patent/TW200706601A/zh
Priority to JP2008514735A priority patent/JP2008542499A/ja
Priority to BRPI0610910-1A priority patent/BRPI0610910A2/pt
Priority to CNA2006800191356A priority patent/CN101185142A/zh
Priority to EP06771441A priority patent/EP1889263A1/en
Priority to KR1020077027795A priority patent/KR20080016823A/ko
Priority to PCT/US2006/020673 priority patent/WO2006130530A1/en
Priority to RU2007144540/09A priority patent/RU2364966C1/ru
Priority to MX2007014925A priority patent/MX2007014925A/es
Priority to ARP060102254A priority patent/AR055961A1/es
Publication of US20060270785A1 publication Critical patent/US20060270785A1/en
Publication of US7902288B2 publication Critical patent/US7902288B2/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L53/00Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C08L53/02Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes
    • C08L53/025Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes modified
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L53/00Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C08L53/02Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J153/00Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
    • C09J153/02Vinyl aromatic monomers and conjugated dienes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J153/00Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
    • C09J153/02Vinyl aromatic monomers and conjugated dienes
    • C09J153/025Vinyl aromatic monomers and conjugated dienes modified
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/10Materials in mouldable or extrudable form for sealing or packing joints or covers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/12Materials for stopping leaks, e.g. in radiators, in tanks
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2666/00Composition of polymers characterized by a further compound in the blend, being organic macromolecular compounds, natural resins, waxes or and bituminous materials, non-macromolecular organic substances, inorganic substances or characterized by their function in the composition
    • C08L2666/02Organic macromolecular compounds, natural resins, waxes or and bituminous materials

Definitions

  • the present invention relates to grease materials for use in connection points of communication cables.
  • the present invention relates to grease materials containing diblock copolymers, which are easy to manufacture and are suitable for protecting communication cables against environmental conditions.
  • Communication cables such as electrical and optical cables, are used in a variety of environmental conditions.
  • communication cables may be placed in humid environments or buried underground.
  • the communication cable needs to withstand water penetration because water can severely affect the performance of the cable.
  • water may destroy the capacitance balance of the electrical conductor, short circuit the electrical cable, and induce high resistance due to corrosion.
  • water may negatively affect the integrity of the optical cable. This is particularly true at connection points of communication cables (e.g., cable boxes and connectors), which are generally more vulnerable to moisture exposure.
  • connection point One solution to minimize water penetration at a connection point involves encasing the communication cables at the connection point, and surrounding the connection point with a water insoluble filling material, such as a grease.
  • a water insoluble filling material such as a grease.
  • the grease generally seals the connection point and stops the migration of water.
  • conventional greases typically used with communication cables are expensive and time consuming to manufacture and exhibit stability issues over extended periods of time. As such, there exists a need for a grease material that is easy to manufacture and is stable for use at connection points communication cables.
  • the present invention is a method of making a sealant material.
  • the method includes providing a diblock copolymer, where the diblock copolymer comprises a plurality of styrene zones and a plurality of rubber zones, and where the styrene zones have a glass transition temperature.
  • the method further includes combining the diblock copolymer with mineral oil at a processing temperature of less than about the glass transition temperature of the styrene zones.
  • the present invention is characterized as a method of making a sealant material, which includes providing a styrene-rubber diblock copolymer, filtering the styrene-rubber diblock copolymer to provide a filtered styrene-rubber diblock copolymer having an average particle size of about one millimeter or less, and immersing the filtered styrene-rubber diblock copolymer in mineral oil at a processing temperature of about 80° C. or less.
  • the present invention is characterized as a sealant material that includes mineral oil and a styrene-rubber diblock copolymer, where the grease material exhibits a blue tint when substantially free of coloring agents.
  • the grease material comprises a gel material.
  • references to a singular compound or composition include both singular and plural forms.
  • a styrene-rubber diblock copolymer refers to one or more styrene-rubber diblock copolymers
  • a styrene-rubber-styrene triblock copolymer refers to one or more styrene-rubber-styrene triblock copolymers.
  • “Styrene zone” means a styrene-rich region of a block copolymer that contains at least about 66% by weight styrene, based on the entire weight of the region.
  • Rubber zone means a rubber-rich region of a block copolymer that contains at least about 66% by weight rubber, based on the entire weight of the region.
  • “Cable” means any type of electrical or optical cable for telecommunications or other use, with any number of wires of fibers, from one up to any desired member.
  • FIG. 1 is a perspective view of a cable box in use with grease material of the present invention and a pair of spliced cables.
  • FIG. 2A is a perspective view of a dropwire connector in use with grease material of the present invention.
  • FIG. 2B is a perspective view of the dropwire connector in use with grease material of the present invention and a pair of wires.
  • FIG. 1 is a perspective view of cable box 10 in use with sealant material 12 , which may comprise a grease material 12 , of the present invention, spliced cables 14 and 16 , and discrete connectors 18 .
  • Cable box 10 is an example of a suitable enclosable container for use with grease material 12 .
  • cable box 10 includes cover members 20 a and 20 b , which are capable of being placed against each other to enclose the internal portions of cable box 10 .
  • Cover member 20 a includes a pair of containment cavities 22 a and 24 a located at the distal ends of cover member 20 a , and a main cavity 26 a disposed between containment cavities 22 a and 24 a .
  • cover member 20 b includes a pair of containment cavities 22 b and 24 b located at the distal ends of cover member 20 b , a main cavity 26 b disposed between containment cavities 22 b and 24 b , and lateral slots 28 and 30 .
  • Spliced cables 14 and 16 extend through the distal ends of cover member 20 b , and are connected with discrete connectors 18 .
  • Grease material 12 of the present invention is disposed in each of containment cavities 22 a , 22 b , 24 a , and 24 b . As such, when cover members 20 a and 20 b are closed together, grease material 12 seals spliced cables 14 and 16 within cable box 10 . This protects the connections between spliced cables 14 and 16 at discrete connectors 18 from external environmental conditions, such as moisture.
  • Grease material 12 compositionally includes mineral oil and a styrene-rubber diblock copolymer, where the diblock copolymer substantially retains significant amounts of rubber chain cross-linking between separate styrene zones of the diblock copolymer (herein referred to as a “physically cross-linked structure”), which is originally provided by the manufacturer.
  • the physically cross-linked structure of the diblock copolymer allows grease material 12 to exhibit good resistance to slumping, even at elevated temperatures. Slumping is an identifying characteristic that a given grease will eventually flow to attain the lowest potential energy state. Slumping and flowing are undesirable traits of grease, especially when used at connection points of communication cables (e.g., cable box 10 ).
  • Grease material 12 of the present invention exhibits good resistance to slumping and does not flow from its original position, even when subjected to temperatures up to or over about 80° C. As such, grease material 12 may continuously provide protection against external environmental conditions over extended periods of time.
  • the physically cross-linked structure of the diblock copolymer is retained by forming grease material 12 at a low processing temperature and/or with shear mixing.
  • the cross-linked structure of the diblock copolymer is temperature and shear dependent. While not wishing to be bound by theory, it is believed that when a styrene-containing diblock copolymer is heated above the glass transition temperature of the styrene zones, the styrene-rich regions of the diblock copolymer reorder and reduce in size. This degrades the rubber chain entanglements and the cross-linked structure. As the cross-linked structure is reduced, the physical cross-linking is correspondingly reduced. This reduces the mechanical strength and resistance to slumping of the resulting grease.
  • the process combines shear mixing with heating above the glass transition temperature of the styrene zones, substantially all of the original cross-linked structure is lost. As such, the resulting grease behaves as a viscous liquid, which flows over time, even at room temperature.
  • Grease material 12 is formed at a processing temperature maintained at less than about the glass transition temperature of the styrene zones of the diblock copolymer, which is generally about 100° C. As such, the diblock copolymer of grease material 12 retains the physically cross-linked structure.
  • Suitable processing temperatures for forming grease material 12 include temperatures of about 80° C. or less, particularly suitable processing temperatures for forming grease material 12 include temperatures of about 50° C. or less, and even more particularly suitable processing temperatures for forming grease material 12 include temperatures of about 30° C. or less.
  • the processing temperature may be maintained at the above-listed temperatures in variety of manners. For example, the mineral oil may be heated to a desired above-listed temperature and maintained while the diblock copolymer and the mineral oil are combined. Alternatively, if the processing temperature is room temperature (i.e., about 25° C.), no heating is required, and the diblock copolymer and the mineral oil may be combined at ambient conditions.
  • the degree of physical cross-linking of the diblock copolymer is temperature and shear dependent.
  • the amount of shear mixing that may be used to form grease material 12 is inversely proportional to the processing temperature.
  • suitable shear mixing levels for forming grease material 12 include low shear levels or less (e.g., no mixing).
  • suitable shear mixing levels for forming grease material 12 include moderate shear levels or less. Examples of moderate shear levels include those produced with propeller or hand paddle mixing, and are sufficient to wet the diblock copolymer particles and distribute them within the mineral oil. This allows grease material 12 to be processed with inexpensive equipment, which reduces processing costs.
  • Grease material 12 is formed by absorbing the mineral oil in the rubber zones of the diblock copolymer without substantially disrupting the styrene zones of the diblock copolymer. This may be accomplished by combining particles of the diblock copolymer with the mineral oil at the suitable processing temperature and/or with shear mixing, as discussed above.
  • the diblock copolymer desirably exhibits a small average particle size to increase the effective surface area in contact with the mineral oil, thereby increasing the rate of absorption.
  • a suitable maximum average particle size for the diblock copolymer prior to combining with the mineral oil is about one millimeter.
  • a particularly suitable maximum average particle size for the diblock copolymer prior to combining with the mineral oil is about 0.5 millimeters.
  • the diblock copolymer is typically purchased as rubbery agglomerate crumbs, which may be readily broken apart to reduce the average particle size of the diblock copolymer. This may be accomplished in a variety of manners.
  • the diblock copolymer may be filtered, in which, as defined herein, the dry diblock copolymer is sifted and pressed through a screen having orifices corresponding to the desired particle sizes.
  • An example of a suitable screen includes a metal screen with a 5.5 wire/centimeter (14-wire/inch) mesh, with 0.023-centimeter (0.009-inch) diameter wires, and which is commercially available from Sefar America, Lumberton, N.J.
  • the screen may be positioned over the mineral oil, which allows the filtered diblock copolymer particles to fall and immerse directly into the mineral oil.
  • the diblock copolymer is also desirably charged to the mineral oil quickly enough so the mineral oil absorbs into the diblock copolymer particles in a substantially uniform manner. This reduces the tendency of the diblock copolymer particles from forming agglomerates. Suitable times for charging the diblock copolymer into the mineral oil include about twenty minutes or less, particularly suitable times for charging the diblock copolymer into the mineral oil include about ten minutes or less, and even more particularly suitable times for charging the diblock copolymer into the mineral oil include about five minutes or less. Portions of the diblock copolymer may be charged continuously or in separate intervals over the given times. If agglomerates of the diblock copolymer particles are formed at the surface of the mineral oil, the agglomerates may be reduced by mixing.
  • the rubber zones of the diblock copolymer absorb the mineral oil until a saturation point is substantially reached.
  • the time required for the rubber zones to become substantially saturated with the mineral oil depends on the temperature of the process and the amount of shear mixing that is applied. As the rubber zones absorb the mineral oil, the viscosity of the resulting mixture increases. As such, an increase in temperature will decrease the time required to form grease material 12 .
  • the resulting grease material 12 appears as a gelatinous material with a visually discernable non-uniform character (i.e., numerous sticky globules that adhere to each other). Additionally, air bubbles may be visually discernable within grease material 12 . The air bubbles are believed to result from air that originates in the diblock copolymer particles, and which is expelled as the rubber zones of the diblock copolymer absorb the mineral oil. The air bubbles may be subsequently removed from grease material 12 by placing grease material 12 under vacuum conditions. If removal of the air bubbles is desired, grease material 12 may be placed under vacuum conditions soon after the diblock copolymer particles are dispersed in the mineral oil.
  • grease material 12 is suitable for use as a grease sealant, and is resistant to slumping, even at elevated temperatures. In one embodiment of the present invention, grease material 12 exhibits substantially no slump when exposed to a temperature of about 80° C. or less when tested pursuant to the Slump Test, discussed below.
  • grease material 12 Another characteristic of grease material 12 is that, after formation, grease material 12 exhibits a blue tint to an unaided human eye at ambient lighting, without the use of coloring agents.
  • Coloring agents are defined herein as any composition, other than the mineral oil or the diblock copolymer, that affects the color of grease material 12 when incorporated.
  • the blue tint is believed to be due to light scattering off of the styrene-rich regions of the diblock copolymer.
  • conventional greases that are formed at processing temperatures at or above the glass transition temperature of the styrene zones of the diblock copolymer are clear, and do not exhibit a blue tint.
  • grease material 12 exhibits a blue tint when tested pursuant to the Copolymer Structure Degradation Test, discussed below.
  • Suitable mineral oils for use in grease material 12 include petroleum distillate hydrocarbon oils, such as paraffinic mineral oils, naphthenic mineral oils, and combinations thereof.
  • Naphthenic mineral oils contain naphthene groups (i.e., cycloparaffin) and are greater than 35% by weight naphthenic and less than 65% by weight paraffinic, according to ASTM D2501-00.
  • Paraffinic mineral oils contain less than 35% by weight naphthenic and greater than 65% by weight paraffinic.
  • suitable commercially available mineral oils include trade designated “KAYDOL” White Mineral Oil and trade designated “SEMTOL 40” White Mineral Oil, both commercially available from Crompton Corporation, Middlebury, Conn.
  • a suitable minimum concentration of the mineral oil in grease material 12 is about 50% by weight, based on the entire weight of grease material 12 .
  • a suitable maximum concentration of the mineral oil in grease material 12 is about 96% by weight, based on the entire weight of grease material 12 .
  • Suitable styrene-rubber diblock copolymers for use in grease material 12 include styrene-isoprene, styrene-polybutadiene, styrene-ethylene/butylene, styrene-ethylene/propylene, and combinations thereof.
  • suitable commercially available diblock copolymers include trade designated “KRATON G1701” and “KRATON G1702” Block Copolymers, both of which are commercially available from Kraton Polymers, Houston, Tex.; and “SEPTON S1020” Block Copolymer commercially available from Septon Company of America, Pasadena, Tex.
  • a suitable minimum concentration of the diblock copolymer in grease material 12 is about 4% by weight, based on the entire weight of grease material 12 .
  • a suitable maximum concentration of the diblock copolymer in grease material 12 is about 15% by weight, based on the entire weight of grease material 12 .
  • the diblock copolymers and mineral oil used in the present invention have similar coefficients of thermal expansion. As such, grease material 12 does not exhibit oil weeping when used at elevated temperatures. Many conventional greases use rheological-modifying agents and oils that have significantly different coefficients of thermal expansion. As such, when the conventional greases are heated in warm environments, the oil separates from the rheological-modifying agents (i.e., weeps). This results in an oily residue on the surface of the conventional grease, which is undesirable.
  • Grease material 12 of the present invention may also include additional components, such as stabilizers, antioxidants, processing aids, styrene-rubber-styrene triblock copolymers, microspheres, silica gels, and combinations thereof.
  • Suitable stabilizers and antioxidants include phenols, phosphites, phosphorites, thiosynergists, amines, benzoates, and combinations thereof.
  • Suitable commercially available phenolic-based antioxidants include trade designated “IRGANOX 1035”, “IRGANOX 1010”, and “IRGANOX 1076” Antioxidants and Heat Stabilizers for wire and cable applications, from Ciba Specialty Chemicals Corp., Tarrytown, N.Y.
  • a suitable maximum concentration of stabilizers or antioxidants in grease material 12 is about 1% by weight, based on the entire weight of grease material 12 .
  • stabilizers and antioxidants may be dissolved or dispersed in the mineral oil prior to combining the diblock copolymer with the mineral oil.
  • Suitable styrene-rubber-styrene triblock copolymers for use in sealant material 12 include styrene-butadiene-styrene (SBS), styrene-isoprene-styrene (SIS), styrene-ethylene/butylene-styrene (SEBS), styrene-ethylene/propylene-styrene (SEPS), and combinations thereof.
  • SBS styrene-butadiene-styrene
  • SEBS styrene-isoprene-styrene
  • SEBS styrene-ethylene/butylene-styrene
  • SEPS styrene-ethylene/propylene-styrene
  • SEBS block copolymers for use in sealant material 12 include trade designated “KRATON G-1650” and “KRATON G-1652” Block Copolymers, both of which are
  • suitable styrene-rubber-styrene triblock copolymers for use in sealant material 12 also include styrene-rubber-styrene triblock copolymers that are included as additives in some commercially available styrene-rubber diblock copolymers.
  • a suitable maximum concentration of the styrene-rubber-styrene triblock copolymer in sealant material 12 includes a concentration ratio of about 1:2, by weight, relative to the styrene-rubber diblock copolymer.
  • the styrene-rubber-styrene triblock copolymer may be mixed with the mineral oil along with the diblock copolymer.
  • Suitable microspheres for use in grease material 12 include functionalized and non-functionalized hollow glass and plastic microspheres.
  • Suitable hollow glass microspheres have average particle sizes, by volume and at effective top size (95%), of about 10 micrometers to about 140 micrometers, and true densities of about 0.1 grams/cubic centimeter (g/cm 3 ) to about 0.4 g/cm 3 .
  • the term “true density” is a concentration of matter, as measured by weight per unit volume.
  • Such hollow glass microspheres contain a large volume fraction of air (e.g., on the order of 90% to 95% air), and exhibit a dielectric constant of about 1.0. As such, hollow glass microspheres reduce the overall dielectric constant of grease material 12 .
  • suitable commercially available hollow glass microspheres for use in grease material 12 include the S Series, K Series, and A Series of trade designated “3M SCOTCHLITE” Glass Bubbles from 3M Company, St. Paul, Minn.
  • suitable 3M SCOTCHLITE Glass Bubbles include 3M SCOTCHLITE K1 Glass Bubbles (true density of 0.125 g/cm 3 ), 3M SCOTCHLITE K15 Glass Bubbles (true density of 0.15 g/cm 3 ), 3M SCOTCHLITE A16 Glass Bubbles (true density of 0.16 g/cm 3 ), 3M SCOTCHLITE K20 Glass Bubbles (true density of 0.20 g/cm 3 ), 3M SCOTCHLITE S22 Glass Bubbles (true density of 0.22 g/cm 3 ), and combinations thereof.
  • a suitable maximum concentration of microspheres in grease material 12 is about 20% by weight, based on the entire weight of grease material 12 .
  • microspheres may be charged to the mineral oil before, after, or currently with combining the diblock copolymer with the mineral oil.
  • grease material 12 is substantially free of petroleum waxes, such as paraffin wax, which are solids at 25° C. Petroleum waxes that exhibit melting points high enough to allow them to contribute to slump resistance typically require high processing temperatures (e.g., 110° C. or greater). Such temperatures are generally greater than the glass transition temperature of the styrene zones of the diblock copolymer. As discussed above, this would reduce the cross-linked structure of the diblock copolymer. Nonetheless, grease material 12 exhibits good resistance to slumping without requiring the use of petroleum waxes.
  • petroleum waxes such as paraffin wax
  • grease material 12 may also be used in a wide variety of applications, such as electrical, opto-electrical (i.e., a combination of optical and electronic components), and optical applications.
  • grease material 12 may also be disposed within discrete connectors 18 , main cavities 26 a and 26 b , and lateral slots 28 and 30 . This provides additional protection to spliced cables 14 and 16 .
  • Additional applications include cables, connectors (e.g., discrete connectors, modular connectors, connector boxes, and grease boxes), and closures (e.g., drop wire closures, filled closures, buried closures, and terminal blocks).
  • An example of a particularly suitable application includes an electrical connector disclosed in Farrar, Jr., U.S. Pat. No. 3,897,129.
  • FIGS. 2A and 2B are perspective views of dropwire connector 32 in use with grease material 12 of the present invention (not shown in FIG. 2A or 2 B).
  • Dropwire connector 32 is an example of a particularly suitable enclosable container for use with grease material 12 .
  • dropwire connector 32 includes connector body 34 , wire openings 36 , body cavity 38 , U-contact 40 , and lid 42 .
  • Wire openings 36 and body cavity 38 extend within connector body 34 , and are substantially filled with grease material 12 .
  • U-contact is disposed in body cavity 38 , and includes slits 44 a and 44 b and slits 46 a and 46 b (slit 46 b not shown in FIG. 2A ).
  • Lid 42 connects to body cavity 38 via living hinge 48 .
  • FIG. 2B shows dropwire connector 32 in use with wires 50 and 52 .
  • wires 50 and 52 may be inserted in wire openings 36 , such that the tips of wires 50 and 52 extend within body cavity 38 .
  • U-contact 40 may then be crimped (i.e., pressed down into body cavity 38 ), which causes wires 50 and 52 to be inserted through slits 44 a and 44 b and slits 46 a and 46 b , respectively.
  • the crimping also strips portions of the insulating layers of wires 50 and 52 , and creates an electrical contact between wires 50 and 52 .
  • Lid 42 may then be closed and secured against connector body 34 , thereby enclosing body cavity 38 .
  • Grease material 12 effectively plugs wire openings 36 and body cavity 38 from external environmental conditions, which protects the connection between wires 50 and 52 against moisture.
  • Grease materials of the present invention were qualitatively measured pursuant to the following procedure to determine which at temperatures the grease materials could continue to exhibit resistance to slumping.
  • the following procedure involves subjecting the grease materials to various temperatures after forming the grease materials. It does not involve varying the processing temperatures for forming the grease materials.
  • a 4-gram sample of the grease material was spread into a 2.54-centimeter (1.00-inch) wide by 0.64-centimeter (0.25-inch) high ointment tin.
  • the tin was then placed in an oven at the desired temperature for a one hour period. After the one hour period, the tin was removed from the oven and allowed to rest at 25° C. for one hour to cool. The tin was then tilted to a vertical orientation, and remained in the vertical orientation for 48 hours. After the 48 hour period, the amount that the grease material moved from its original position was visually examined and ranked on a scale of 1-4. Table 1 provides the scale rankings and their corresponding criteria.
  • Grease materials of the present invention were qualitatively measured pursuant to the following procedure to determine the extent of degradation of the cross-linked structure of the diblock copolymer.
  • grease materials that retain physically cross-linked structures of the diblock copolymer exhibit a blue tint due to light scattering off of the styrene-rich regions of the diblock copolymer.
  • the cross-linked structure of the diblock copolymer degrades, such as when the grease materials are heated near or above the glass transition temperature of the styrene zones of the diblock copolymer, the blue tint disappears.
  • whether or not a grease material exhibits a blue tint is indicative of whether or not the grease material was subjected to high temperatures when formed, or subsequently.
  • a 250-gram sample of the grease material was visually examined in a clear 16-ounce jar to see whether or not the grease material exhibited a blue tint to an unaided human eye at ambient lighting.
  • the presence of a blue tint is evidence that the grease material was not formed at processing temperatures near or above the glass transition temperature of the styrene zones of the diblock copolymer.
  • the sample size used in this test provides an adequate amount of grease material to provide the blue tint, if present. Smaller sample sizes may not exhibit the blue tint due to the smaller amounts of light scattering. This effect is similar to the light scattering of water (i.e., a small cup of water appears clear, while a large lake of water appears blue).
  • Table 2 provides the amounts of the mineral oil and the diblock copolymer used for each Example, and the weight percent of the diblock copolymer in the grease material.
  • Example Copolymer Diblock Copolymer (grams) (grams) (grams) (grams)
  • Example 1 G1702 6.0% 15 235
  • Example 2 G1702 8.0% 20
  • Example 3 G1702 10.0% 25 225
  • Example 4 G1701 10.0% 25 225
  • Example 5 S1020 10.0% 25 225
  • Example 6 G1701 12.5% 31 219
  • Example 7 S1020 12.5% 31 219
  • the given amount of Kaydol oil was poured into a 16-ounce jar and continually mixed. The mixing was performed at 500 rotations-per-minute with a three-bladed steel propeller and a Model 2AM-NCC-16 air motor from Gast Manufacturing Corp., Benton Harbor, Mich.
  • the Kaydol oil was mildly heated and 0.2% by weight (based on the entire weight of the grease material) of Irganox antioxidant was dissolved in the Kaydol oil.
  • the processing temperature was then reduced to, and maintained at 25° C. (i.e., no heating) and atmospheric pressure.
  • the diblock copolymer was then filtered and charged to the jar in a five minute period.
  • the diblock copolymer was filtered with a 5.5-wire/centimeter mesh screen having an orifice diameter of 0.157 centimeters (0.062 inches). The screen was placed over the jar so that the diblock copolymer fell directly into the mixing mineral oil.
  • the mineral oil and diblock copolymer were then mixed in the jar at 25° C. and atmospheric pressure for an additional five minutes at the same mixing speed. After the five minute period, the mixing was stopped and the jar containing the resulting grease material was placed in a vacuum maintained at 30 mmHg until the grease material foamed. The jar was then removed from the vacuum and the grease material was allowed to rest at 25° C. and atmospheric pressure for 12 hours. The grease material was then visually examined pursuant to the Copolymer Structure Degradation Test, discussed above. After formation, each of the grease materials of Examples 1-7 exhibited a blue tint. As such, the grease materials retained physically cross-linked structures of their diblock copolymers after formation.
  • Example 1 4 (none) 3 (minor) 3 (minor) 3 (minor)
  • Example 2 4 (none) 3 (minor) 3 (minor) 3 (minor)
  • Example 3 4 (none) — 4 (none) 3 (minor)
  • Example 4 4 (none) — 4 (none) 4 (none)
  • Example 5 4 (none) — 4 (none) 4 (none)
  • Example 6 4 (none) — 4 (none) 4 (none)
  • Example 7 4 (none) — 4 (none) 4 (none)
  • Example 1 3 (minor) 1 (severe) 1 (severe) 1 (severe)
  • Example 2 3 (minor) 2 (moderate) 1 (severe) 1 (severe)
  • Example 3 3 (minor) 3 (minor) 1 (severe) 1 (severe)
  • Example 4 3 (minor) 3 (minor) 2 (mod- erate)
  • Example 5 4 (none) 2 (moderate) 2 (moderate) —
  • Example 6 4 (none) 4 (none) 3 (minor) 2 (mod- erate)
  • Example 7 4 (none) 4 (none) 2-3 (minor-moderate) 1 (severe)
  • the grease materials of Examples 1-7 were visually examined again pursuant to the Copolymer Structure Degradation Test, discussed above.
  • the grease materials of the present invention are particularly suitable for uses at these temperatures.
  • the grease materials of Examples 3-7 were not tested at 80° C. However, due to the higher concentrations of diblock copolymer in the grease materials of Examples 3-7, it is believed that such grease materials would also have exhibited a blue tint.
  • the grease materials of Examples 1-7 were also subjected to a modified Slump Test. In this test, after each tin was removed from the oven and allowed to rest at 25° C. for one hour to cool, the tin was then tilted to a vertical orientation, and remained in the vertical orientation for four days (rather than 48 hours). Any grease materials that exhibited slump at this point were removed from the remainder of this test. The tins with the remaining grease materials were then placed in a 70° C. oven and in an 80° C. oven for one hour at a vertical orientation.
  • Table 5 provides the scaled rankings of the amounts of slumping the grease materials exhibited when exposed to the 70° C. environment.
  • Table 6 provides the scaled rankings of the amounts of slumping the grease materials exhibited when exposed to the 80° C. environment.
  • Example 1 4 (none) N/T N/T N/T N/T
  • Example 2 4 (none) N/T N/T N/T N/T
  • Example 3 4 (none) 4 (none) N/T N/T N/T
  • Example 4 4 (none) 4 (none) 4 (none) 3 (minor) N/T
  • Example 5 4 (none) 4 (none) 4 (none) 4 (none) N/T
  • Example 6 4 (none) 4 (none) 4 (none) 4 (none) 4 (none)
  • Example 7 4 (none) 4 (none) 4 (none) 4 (none) (none) (N/T)
  • Example 5 4 (none) 4 (none) 4 (none) 4 (none) N/T
  • Example 7 4 (none) 4 (none) 4 (none) 4 (none) (none) (N/T) Not tested

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Lubricants (AREA)
  • Sealing Material Composition (AREA)
US11/141,137 2005-05-31 2005-05-31 Sealant materials containing diblock copolymers and methods of making thereof Expired - Fee Related US7902288B2 (en)

Priority Applications (11)

Application Number Priority Date Filing Date Title
US11/141,137 US7902288B2 (en) 2005-05-31 2005-05-31 Sealant materials containing diblock copolymers and methods of making thereof
KR1020077027795A KR20080016823A (ko) 2005-05-31 2006-05-30 이중 블록 공중합체를 함유하는 실란트 재료 및 그 제조방법
RU2007144540/09A RU2364966C1 (ru) 2005-05-31 2006-05-30 Уплотнительные материалы, содержащие диблочные сополимеры, и способы их создания
BRPI0610910-1A BRPI0610910A2 (pt) 2005-05-31 2006-05-30 materiais selantes contendo copolÍmeros dibloco e mÉtodos de fabricaÇço desses
CNA2006800191356A CN101185142A (zh) 2005-05-31 2006-05-30 含有二嵌段共聚物的密封材料及其制备方法
EP06771441A EP1889263A1 (en) 2005-05-31 2006-05-30 Sealant materials containing diblock copolymers and methods of making thereof
TW095119283A TW200706601A (en) 2005-05-31 2006-05-30 Sealant materials containing diblock copolymers and methods of making thereof
PCT/US2006/020673 WO2006130530A1 (en) 2005-05-31 2006-05-30 Sealant materials containing diblock copolymers and methods of making thereof
JP2008514735A JP2008542499A (ja) 2005-05-31 2006-05-30 二元ブロック共重合体を含有するシーラント材料及びその製造方法
MX2007014925A MX2007014925A (es) 2005-05-31 2006-05-30 Materiales de sellado que contienen copolimeros dibloque y metodos para su fabricacion.
ARP060102254A AR055961A1 (es) 2005-05-31 2006-05-31 Materiales de sellado con copolimeros dibloque y metodos para su fabricacion

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Application Number Priority Date Filing Date Title
US11/141,137 US7902288B2 (en) 2005-05-31 2005-05-31 Sealant materials containing diblock copolymers and methods of making thereof

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US7902288B2 true US7902288B2 (en) 2011-03-08

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EP (1) EP1889263A1 (pt)
JP (1) JP2008542499A (pt)
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CN (1) CN101185142A (pt)
AR (1) AR055961A1 (pt)
BR (1) BRPI0610910A2 (pt)
MX (1) MX2007014925A (pt)
RU (1) RU2364966C1 (pt)
TW (1) TW200706601A (pt)
WO (1) WO2006130530A1 (pt)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8585430B1 (en) 2012-04-05 2013-11-19 Google Inc. Connector with a severing device and wire taps

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7883608B2 (en) * 2006-11-07 2011-02-08 The Patent Store Llc Cathodic protection systems
WO2010042422A2 (en) * 2008-10-07 2010-04-15 3M Innovative Properties Company Composition, method of making the same, and use thereof
US20110174365A1 (en) * 2010-01-18 2011-07-21 Drake Kenneth C System and method for forming roofing solar panels
WO2013032654A1 (en) * 2011-08-29 2013-03-07 3M Innovative Properties Company Sealant materials and methods of using thereof

Citations (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3683104A (en) 1971-01-07 1972-08-08 Dow Chemical Co Heat resistant cable
US3879575A (en) 1974-02-21 1975-04-22 Bell Telephone Labor Inc Encapsulating compound and closure
US3897129A (en) 1973-09-26 1975-07-29 Minnesota Mining & Mfg Connector encapsulating device and method
US4176240A (en) 1978-05-30 1979-11-27 Bell Telephone Laboratories, Incorporated Filled electrical cable
US4324453A (en) 1981-02-19 1982-04-13 Siecor Corporation Filling materials for electrical and light waveguide communications cables
US4333706A (en) 1979-12-26 1982-06-08 Siecor Corporation Filling materials for communications cable
US4351913A (en) 1981-02-19 1982-09-28 Siecor Corporation Filling materials for electrical and light waveguide communications cables
EP0067009A1 (en) 1981-05-26 1982-12-15 RAYCHEM CORPORATION (a California corporation) Water-excluding filling composition
US4464013A (en) 1982-03-29 1984-08-07 At&T Bell Laboratories Filled optical fiber cables
US4497538A (en) 1983-08-10 1985-02-05 Siecor Corporation Filled transmission cable
US4509821A (en) 1981-09-10 1985-04-09 Sun Tech, Inc. Filling material for electric cable
US4617422A (en) 1981-01-30 1986-10-14 Bicc Public Limited Company Electric cables and compositions for use in them
US4639483A (en) 1985-05-09 1987-01-27 Minnesota Mining And Manufacturing Company Soap-thickened reenterable gelled encapsulants
US4701016A (en) 1985-01-31 1987-10-20 American Telephone And Telegraph Company, At&T Bell Laboratories Thixotropic grease composition and cable comprising same
US4798853A (en) 1984-12-28 1989-01-17 Shell Oil Company Kraton G thermoplastic elastomer gel filling composition for cables
EP0299718A2 (en) 1987-07-13 1989-01-18 Raychem Corporation Heat-resistant gel compositions
US5187763A (en) 1991-04-26 1993-02-16 American Telephone & Telegraph Company Optical fiber cable having dripless, non-bleeding and optical fiber coating-compatible waterblocking material in core thereof
WO1993005113A1 (en) 1991-09-06 1993-03-18 Raychem Limited Gels
US5262468A (en) 1977-03-17 1993-11-16 Applied Elastomerics, Inc. Thermoplastic elastomer gelatinous compositions
US5360350A (en) 1991-08-23 1994-11-01 The Whitaker Corporation Sealant compositions and sealed electrical connectors
US5657410A (en) 1993-05-13 1997-08-12 Siemens Aktiengesellschaft Filler for an optical transmission element having at least one optical waveguide
EP0889343A2 (en) 1997-07-01 1999-01-07 Lucent Technologies Inc. Optical fiber cable having an improved filling material within its core
WO2001074480A1 (en) * 2000-03-31 2001-10-11 Unigel Limited Gel compositions
US20020007002A1 (en) * 1996-08-12 2002-01-17 Sebastian Plamthottam S-EB-S block copolymer/oil aqueous dispersion and its use in forming articles
US20020013402A1 (en) * 2000-03-21 2002-01-31 Fisher Dennis Keith Lap edge roofing sealant
US6374023B1 (en) 1999-05-28 2002-04-16 Corning Cable Systems Llc Communication cable containing novel filling material in buffer tube
EP1197971A1 (en) 2000-10-10 2002-04-17 Dynasol Elastomeros, S.A. Composition for cables filling
US20030039621A1 (en) * 2001-04-10 2003-02-27 L'oreal Two-coat make-up product, its use and a kit containing the make-up product
WO2005045852A1 (en) 2003-10-28 2005-05-19 3M Innovative Properties Company Cable filling materials
US20060045895A1 (en) * 2000-11-15 2006-03-02 L'oreal S.A. Cosmetic composition comprising a polymer particle dispersion and a pigment dispersion

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58196244A (ja) * 1982-05-12 1983-11-15 Mitsubishi Petrochem Co Ltd エラストマ−への軟化剤の添加方法
US5201499A (en) * 1991-08-28 1993-04-13 Bridgestone/Firestone, Inc. Fabric reinforced stiffener for air springs

Patent Citations (33)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3843568A (en) 1971-01-07 1974-10-22 Dow Chemical Co Heat resistant compositions
US3683104A (en) 1971-01-07 1972-08-08 Dow Chemical Co Heat resistant cable
US3897129A (en) 1973-09-26 1975-07-29 Minnesota Mining & Mfg Connector encapsulating device and method
US3879575A (en) 1974-02-21 1975-04-22 Bell Telephone Labor Inc Encapsulating compound and closure
US5262468A (en) 1977-03-17 1993-11-16 Applied Elastomerics, Inc. Thermoplastic elastomer gelatinous compositions
US4176240A (en) 1978-05-30 1979-11-27 Bell Telephone Laboratories, Incorporated Filled electrical cable
US4333706A (en) 1979-12-26 1982-06-08 Siecor Corporation Filling materials for communications cable
US4617422A (en) 1981-01-30 1986-10-14 Bicc Public Limited Company Electric cables and compositions for use in them
US4351913A (en) 1981-02-19 1982-09-28 Siecor Corporation Filling materials for electrical and light waveguide communications cables
US4324453A (en) 1981-02-19 1982-04-13 Siecor Corporation Filling materials for electrical and light waveguide communications cables
EP0067009A1 (en) 1981-05-26 1982-12-15 RAYCHEM CORPORATION (a California corporation) Water-excluding filling composition
US4509821A (en) 1981-09-10 1985-04-09 Sun Tech, Inc. Filling material for electric cable
US4464013A (en) 1982-03-29 1984-08-07 At&T Bell Laboratories Filled optical fiber cables
US4497538A (en) 1983-08-10 1985-02-05 Siecor Corporation Filled transmission cable
US4798853A (en) 1984-12-28 1989-01-17 Shell Oil Company Kraton G thermoplastic elastomer gel filling composition for cables
US4701016A (en) 1985-01-31 1987-10-20 American Telephone And Telegraph Company, At&T Bell Laboratories Thixotropic grease composition and cable comprising same
US4639483A (en) 1985-05-09 1987-01-27 Minnesota Mining And Manufacturing Company Soap-thickened reenterable gelled encapsulants
EP0299718A2 (en) 1987-07-13 1989-01-18 Raychem Corporation Heat-resistant gel compositions
US5187763A (en) 1991-04-26 1993-02-16 American Telephone & Telegraph Company Optical fiber cable having dripless, non-bleeding and optical fiber coating-compatible waterblocking material in core thereof
US5360350A (en) 1991-08-23 1994-11-01 The Whitaker Corporation Sealant compositions and sealed electrical connectors
US5741843A (en) * 1991-08-23 1998-04-21 The Whitaker Corporation Sealant compositions and sealed electrical connectors
US5541250A (en) 1991-09-06 1996-07-30 Raychem Limited Gels
WO1993005113A1 (en) 1991-09-06 1993-03-18 Raychem Limited Gels
US5657410A (en) 1993-05-13 1997-08-12 Siemens Aktiengesellschaft Filler for an optical transmission element having at least one optical waveguide
US20020007002A1 (en) * 1996-08-12 2002-01-17 Sebastian Plamthottam S-EB-S block copolymer/oil aqueous dispersion and its use in forming articles
EP0889343A2 (en) 1997-07-01 1999-01-07 Lucent Technologies Inc. Optical fiber cable having an improved filling material within its core
US6374023B1 (en) 1999-05-28 2002-04-16 Corning Cable Systems Llc Communication cable containing novel filling material in buffer tube
US20020013402A1 (en) * 2000-03-21 2002-01-31 Fisher Dennis Keith Lap edge roofing sealant
WO2001074480A1 (en) * 2000-03-31 2001-10-11 Unigel Limited Gel compositions
EP1197971A1 (en) 2000-10-10 2002-04-17 Dynasol Elastomeros, S.A. Composition for cables filling
US20060045895A1 (en) * 2000-11-15 2006-03-02 L'oreal S.A. Cosmetic composition comprising a polymer particle dispersion and a pigment dispersion
US20030039621A1 (en) * 2001-04-10 2003-02-27 L'oreal Two-coat make-up product, its use and a kit containing the make-up product
WO2005045852A1 (en) 2003-10-28 2005-05-19 3M Innovative Properties Company Cable filling materials

Non-Patent Citations (7)

* Cited by examiner, † Cited by third party
Title
KRATON® Thermoplastic Rubber 519-86.
Technical Bulletin Shell Chemical Company, SC:1102-89 KRATON® Thermoplastic Rubbers in Oil Gels.
Technical Bulletin Shell Chemical Company, SC:72-78, Solution Behavior of KRATON® G Thermoplastic Rubber.
Technical Bulletin Shell Chemical Company, SC:759-89, Kraton® G 1701 Thermoplastic Rubber.
Technical Bulletin Shell Chemical Company, SC:972-87, Kraton® G Rubbers in Clear Sealants.
U.S. Application entitled "Filling Materials", filed Dec. 17, 2004, having U.S. Appl. No. 11/015,047.
U.S. Application entitled "Filling Materials", filed Jan. 27, 2004, having U.S. Appl. No. 60/539,521.

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8585430B1 (en) 2012-04-05 2013-11-19 Google Inc. Connector with a severing device and wire taps
US9214778B1 (en) 2012-04-05 2015-12-15 Google Inc. Method for placing an intermediate device in series with at least one wire

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WO2006130530A1 (en) 2006-12-07
JP2008542499A (ja) 2008-11-27
US20060270785A1 (en) 2006-11-30
CN101185142A (zh) 2008-05-21
RU2007144540A (ru) 2009-07-20
TW200706601A (en) 2007-02-16
BRPI0610910A2 (pt) 2008-12-02
AR055961A1 (es) 2007-09-12
EP1889263A1 (en) 2008-02-20
MX2007014925A (es) 2008-02-14
RU2364966C1 (ru) 2009-08-20
KR20080016823A (ko) 2008-02-22

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